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JOURNAL OF APPLIED PHYSICS 106, 073511 2009

Inuence of temperature and excitation procedure on the athermal behavior of Nd3+-doped phosphate glass: Thermal lens, interferometric, and calorimetric measurements
N. G. C. Astrath,1,a M. J. Barboza,1 A. N. Medina,1 A. C. Bento,1 M. L. Baesso,1,b W. F. Silva,2 C. Jacinto,2 and T. Catunda3
1 2

Departamento de Fsica, Universidade Estadual de Maring, 87020-900 MaringPR, Brazil Instituto de Fsica, Universidade Federal de Alagoas, 57072-970 MaceiAL, Brazil 3 Instituto de Fsica de So Carlos, Universidade de So Paulo, 13560-970 So CarlosSP, Brazil

Received 9 June 2009; accepted 24 August 2009; published online 12 October 2009 In this work, thermal and optical properties of the commercial Q-98 neodymium-doped phosphate glass have been measured at low temperature, from 50 to 300 K. The time-resolved thermal lens spectrometry together with the optical interferometry and the thermal relaxation calorimetry methods were used to investigate the glass athermal characteristics described by the temperature coefcient of the optical path length change, ds / dT. The thermal diffusivity was also determined, and the temperature coefcients of electronic polarizability, linear thermal expansion, and refractive index were calculated and used to explain ds / dT behavior. ds / dT measured via thermal lens method was found to be zero at 225 K. The results provided a complete characterization of the thermo-optical properties of the Q-98 glass, which may be useful for those using this material for diode-pumped solid-state lasers. 2009 American Institute of Physics. doi:10.1063/1.3234396
I. INTRODUCTION

Since the advent of lasers in the 1960s, glass materials have been extensively used in the development of resonant cavities.110 Either as highly transparent optical windows or mostly as host for luminescent ions. Optical glasses have also been used for high power lasers. The key point in designing an efcient conventional solid-state laser system is to minimize the beam distortion caused by thermal effects caused by the nonradiative decay processes that take place in the host. As a result, a transverse temperature eld is established inducing a refractive index gradient behaving like an optical lensthe thermal lens TL effect. Moreover, it can also induce surface deformation/displacement, depolarization losses, and material fractures.5,11,12 In other words, it is often considered as the ultimate limitation for power scaling.13 On the other hand, as demonstrated in recent studies performed in doped dielectric microchip lasers, the TL plays a vital role in stabilizing the plane-plane cold cavity and hence enabling high quality laser output.13,14 This reinforces the importance of quantitative evaluation of the TL effect in laser materials. The average power in solid-state lasers is limited primarily by thermo-optic effects in the solid-state gain medium. These effects include stress fracture, stress-induced birefringence, and thermo-optic distortion of the gain element. Desired properties of the gain medium include high thermal conductivity k , low temperature coefcient of the optical path length change ds / dT , and high luminescence quantum . For instance, ds / dT is related to the optical efciency beam distortion. It has different denitions depending on the excitation source prole and the optical system design. When
a b

Electronic mail: astrathngc@pq.cnpq.br. Author to whom correspondence should be addressed. Electronic mail: mlbaesso@pq.cnpq.br.

a uniformly distributed temperature rise occurs as in the case of most high power ashlamp/arclamp pumped solid-state lasers, ds / dT depends on the temperature coefcients of refractive index and thermal expansion. When the hosts are nonuniformly excited, as occurs for laser pumped sources, this parameter includes the sample surface bulging as a consequence of the localized induced temperature rise in the active medium.13,14 Then, it is necessary to combine different techniques to provide the absolute values of this parameter according to the used excitation characteristics. Phosphate glasses have been widely used as matrices for laser applications. When doped with Nd3+, it presents high luminescence quantum efciency .7 In fact, they are the most common laser glass produced nowadays,15 operating in the power regime up to terawatt.10 In such high power domain, it is crucial to control the active medium temperature, what is directly related to the material thermo-optical properties. The quantitative determination of the thermal and optical properties of these glasses as a function of temperature is fundamental for both their structural characterization and optical system optimization. TL spectrometry TLS has been applied to characterize several kinds of materials in a wide temperature range, from 4 to 800 K.1621 Besides the thermal diffusivity D values, combining the data measured with this method with those by optical interferometry OI Ref. 22 and thermal relaxation calorimetry TRC ,23 a general picture about the material thermo-optical properties can be obtained, such as the values of ds / dT, k, and . Therefore, in this work we measured the thermo-optical properties of the commercial Q-98 neodymium-doped phosphate glass and what was performed in the low temperature region, from 50 to 300 K. Athermal characteristics were observed for this glass around 225 K. The TLS was used, to 2009 American Institute of Physics

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Excitation laser Ar+ - 514nm

M1 Shutter L1 M3

Probe laser HeNe - 632.8nm Digital scope

The temporal TL transient depends on the characteristic TL time constant tc, which is related to the thermal diffusiv2 ity D by tc = oe / 4D. The parameter is the probe beam phase shift induced by the TL and can be written as = Pabs ds k p dT .
TL

L2
Sample
Temperature Controller Liquid-He Cooler unity

PC

Signal

P2
Trigger

Pinhole M5

M6 M4

Windows

M2

P1
FIG. 1. TL experimental setup. The excitation and probe beams are proand a HeNe laser vided by an Ar+ ion laser e = 514 nm P = 632.8 nm , respectively. M i, Li, and Pi correspond to mirrors, lenses, and photodiodes, respectively. The windows are quartz disks.

Here, p is the probe beam wavelength and ds / dT TL is the temperature coefcient of the optical path length change at the probe beam wavelength. We added the subscript TL in order to specify that it is measured with the TL data. This is the case of nonuniform excitation, which results to bulging in the sample surface as a consequence of the localized temperature rise induced by the excitation laser beam.12,15 ds / dT TL can be written as9

gether with the OI and TRC methods, to quantify D, k, the temperature coefcients of refractive index dn / dT , electronic polarizability , and ds / dT.

dn 1 3 ds + n Y T (qll + q ) = ( n 1)(1 + ) T + dT 4 dT TL

II. EXPERIMENTAL AND TECHNIQUES DETAILS

The sample investigated in this work is a commercial phosphate glass, namely Q-98, from Kigre Inc., doped with 1 wt % of Nd2O3. A schematic representation of the TL dual beam mode-mismatched experimental conguration is depicted in Fig. 1.11,17 In this setup, a probe laser beam propagates through the TL sensing the generated optical element, which changes its on-axis intensity, I t . The detection of the TL signal was performed by a silicon photodiode P2 , connected to a digital scope. For the measurements as a function of temperature, the sample was cooled at 50 K by He exchange in a continuous ow cryostat Janis, ST-100 , and a Lakeshore temperature controller model 32101 was used to stabilize the temperature. Highly transparent quartz disks were used to seal the Dewar chamber, as shown in Fig. 1. A HeNe laser operating at P = 632.8 nm and an Ar+ ion laser at e = 514 nm were used as probe and excitation beams, respectively. Exposure of the sample to the excitation beam was controlled by means of a shutter. About 10 excitation beam shots were used to average the nal TL transient. In the cw excitation regime, the TL theoretical model provides a simple and analytical expression that links thermo-optical properties of the sample to the time resolved TL transient signal, which is given by1118 It = 1 tan1 I0 2 2mV 2 2 1 + 2m + V tc/2t + 1 + 2m + V2
2

Here, is the Poissons ratio, T is the linear thermal expansion coefcient, dn / dT is the temperature coefcient of refractive index, Y is the Youngs modulus, and qll and q are the stress-optical coefcients parallel and perpendicular to the beam direction, respectively. The rst term in Eq. 3 represents the end-face curvature due to the larger expansion of the excited region hotter center as compared to the edge of the sample. As a consequence the cooler part of the sample prevents expansion of the mentioned hotter center, then thermal stress can be generated, which is what is given by the third term in Eq. 3 . Generally, this term is much smaller than the two previous ones and can be omitted.15 The terms 1 + and the stress-optical coefcients appear in Eq. 3 due to the lenslike shape of TL temperature prole. The parameter is the fraction of the absorbed energy that is converted into heat. Pabs is the absorbed pump power, which can be determined by11 Pabs = Pin 1 R 1 exp AeL . 1 R exp AeL 4

, 1

in which m = 1p / 0e 2 and V = Z1 / Zc. Zc is the confocal distance of the probe beam, Z1 is the distance between the probe beam waist and the sample, 1p and 0e are respectively the probe and excitation beams radii at the sample position, and I 0 = I t when the transient time t or is zero. In this work, we used 0e = 37.8 m, m = 40.1, and V = 2.7 measured as described in Ref. 18 .

Pin is the input power of the excitation laser beam, R is the Fresnel reectivity, Ae is the optical absorption coefcient at the excitation wavelength, and L is the sample thickness. The denominator of the Pabs equation accounts for the multiple internal reections of the pump beam within the sample.11 The values of Ae were obtained by measuring the transmittance of the samples as a function of temperature in the same TL setup, while the reectivity as a function of temperature was determined from refractive index data obtained from the literature.15 For the neodymium-doped samples, the thermal loading, i.e., the fraction of the absorbed energy converted into heat, is provided by = 1 e / em , in which em is the average emission wavelength. We also applied the OI technique to determine, from 120 to 430 K, the temperature dependence of ds / dT OI. In this method the sample is uniformly heated and then the subscript OI species ds / dT measured in such condition. In this technique, the reections of a weak HeNe laser beam 632 nm from both sample surfaces interfere creating interference

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I(t)/I(0), Normalized TL signal (au)

D (10 cm /s)

D (10 cm /s)

1.00

D=(2.30.1)x10 cm /s -1 /Pin=-(0.1220.003) W

-3

-3

1.02

T=300K (ds/dT)TL>0

10.0

(a)
6 4

Pin=200mW

7.5

-3

-0.560.02

-0.770.02

5.0

100

200

300

Temperature (K)

2.5

0.98 Pin=350mW
3.0
-3 2

(ds/dT)TL<0

/Pabs (W )

T=100K (ds/dT)TL<0 0.94 0 10 20

-1

0.96

D=(4.70.1)x10 cm /s
/Pin=(0.2450.009) W
-1

1.5 0.0 -1.5

30

40
-3.0

(b)
50 100 150 200

(ds/dT)TL>0 250 300

Time (ms)
FIG. 2. Normalized TL signal I t / I 0 300 K. for the Q-98 glass at 100 and

Temperature (K)
FIG. 3. Values of D T and / PABS T of the Q-98 glass. The inset in a presents D T in logarithmic scales.

fringes. Using a heating device, a slow and uniform variation in the temperature can be induced in the whole sample, causing the fringes to move. Thus a temperature dependent interferogram can be obtained and used to calculate ds / dT OI. Details of the experimental procedure of this method can be found in Ref. 22. It is important to reinforce that in this procedure this parameter is obtained taking in account the beam phase shift after being reected in the two surfaces of the sample. It can be written as22 ds dT =
OI

dn +n dT

T.

It is convenient here to differentiate this denition for ds / dT OI from that usually found in the literature to describe the ds / dT in laser hosts when a uniformly distributed temperature rise occurs, as in the case of most high power ashlamp/arclamp pumped solid-state lasers, i.e., ds dT = dn + n1 dT
T,

in which n is the refractive index at the respective temperature. In this case the beam phase shift is taken into account considering that it is transmitted though the sample and not via reection in the two surfaces as the case of ds / dT OI. A Quantum design Physical Property Measurement System PPMS and a homemade thermal relaxation23 calorimeters were used to measure the specic heat from 2 to 150 K and from 150 to 470 K, respectively.

III. RESULTS AND DISCUSSION

Figure 2 shows two examples of normalized TL transient for the Q-98 sample at 100 and 300 K, with Pin = 350 mW and Pin = 200 mW, respectively. At 300 K, the optical element created in the sample converges the probe beam leading the signal at the detector to increase. This behavior is expected for materials with ds / dT TL 0. On the other

hand, in the low temperature region the transient displays the divergent nature of the TL optical element, characteristic of ds / dT TL 0. The continuous lines in Fig. 2 correspond to the least square curve tting using Eq. 1 , which provided the values of the TL characteristic time response tc as 1.54 0.03 ms at 300 K and 0.76 0.03 ms at 100 K, and the probe beam / Pin, as 0.122 phase shift normalized by Pin, 0.003 W1 at 300 K and 0.245 0.009 W1 at 100 K. The temperature dependence of tc and / Pin was obtained by performing the acquisition of the TL transients ranging from 50 to 300 K. The thermal diffusivity can be 2 directly calculated using D = oe / 4tc. Figure 3 a presents D T values, which decrease with increasing temperature, varying from 6.9 0.3 103 cm2 / s at 50 K to 2.3 0.1 103 cm2 / s at 300 K. It also shows two regimes, varying with T0.56 0.02 below 130 K and with T0.77 0.02 afterward, as shown in log-log plot in the inset of Fig. 3 a . Figure 3 b shows the normalized TL phase shift, / Pabs T . Since the refractive index variation in this temperature range is very small,15 we considered Ae and R constant and equal to their respective values at room temperature. Then, Pabs T was calculated. It is interesting to note that / Pabs T presents positive values below 225 K, it means ds / dT TL 0, and negative ones above 225 K, i.e., ds / dT TL 0. As observed for other glasses,11,17 D T values eventually reach a constant value as the temperature is increased. The thermal diffusivity depends on the average sound velocity s and the phonon mean free path as D = 1 / 3 vs . At moderate low temperature, the number of phonons involved in anharmonic scattering is proportional to T, resulting in an increase in the mean free path as the temperature decreases with a T1 dependence.11,24,25 Therefore, the results presented here indicate that the mean free path is not the unique quantity driving D in the low temperature range. D T , therefore, reects the variation in both the mean free path and the sound velocity. This happens due to the fact that at high

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(a)

(b)

0.9

(a)
(ds/dT)TL

225K

320K

ds/dT (10 K )

-1

cp/T (Jg K )

10

-4

-1

-1

-6

K (10 Wcm K )

TM=11.2 K

-6

0.0 -0.9 -1.8 -2.7 12

-1

(ds/dT)*(T)=dn/dT(T)+[n(T)-1]T(T)

-3

(ds/dT)OI (10 K )

10

-7

(b)

-1

2 10 100 100 200 300

-6

10 8 6 4

Temperature (K)

Temperature (K)

FIG. 4. Temperature dependence of a the specic heat in the c p / T3 scale and b k T of the Q-98 glass.

50

100

150

200

250

300

350

400

450

Temperature (K)
FIG. 5. Temperature dependence of the temperature coefcient of optical path length a open circles measured via TL method ds / dT TL and open squares calculated using ds / dT T = dn / dT T + n T 1 T T and b measured by OI ds / dT OI method. The uncertainty in ds / dT TL and ds / dT OI determination is less than 15% and 5%, respectively.

temperatures the mean free path in amorphous materials coincides with the interatomic separation, whereas the bonding forces between two neighboring atoms drive the sound velocity.11 Figure 4 a shows the specic heat of the Q-98 sample in c p / T3 scale. It presents a bump at the temperature called TM , T M = 11.2 K. This is the anomalous behavior that is well known to occur in the specic heat of glasses at low temperature.2530 It is not expected to happen in materials that obey the Debye law-crystalline solids. It is driven by the presence of additional phonon states in the glassy system. It has also been reported as a bump in the phonon spectrum, commonly referred as the boson peak, which is obtained from the plot of the number of phonon against their respective frequency.29 The values of k T were calculated using the relation k = D c p, using D T and c p T data. The thermal expansion coefcient of this glass is approximately 1 105 K1 Ref. 15 at room temperature, and even lower at low temperature, which causes the sample total volume to change less than 1% during the considered temperature interval. Thus, the mass density = 3.1 g / cm3 Ref. 15 is assumed to have a negligible variation with the increasing temperature. Figure 4 b shows the k T from 50 to 300 K. k T values increase from 2.6 0.1 103 W / cm K at 50 K to 5.0 0.1 103 W / cm K at 300 K. Once for this glass can be calculated from the luminescence quantum efciency of the 4F3/2 Nd3+ level previously determined at room temperature,15 as = 0.91 0.05, ds / dT TL can be obtained using Eq. 2 . Although values are expected to be higher as the temperature is decreased, as shown in Ref. 17 for the Nd3+ doped aluminosilicate glasses, this high value for this glass at room temperature indicates that the mentioned variation may not be signicant. Then, we assumed T constant in the temperature range of the experiments, resulting in = 0.57 0.04. This introduces additional uncertainty in , but allows to calculate ds / dT TL. Thus, using k T and / Pabs T , ds / dT TL T was calculated, as shown in Fig. 5 a . For comparison, Fig. 5 b shows ds / dT OI T measured via the OI method. In addition, Fig. 5 a shows ds / dT

calculated with the expression ds / dT T = dn / dT T + n T 1 T T used to describe it in laser hosts when a uniformly distributed temperature rise occurs, as in the case of most high power ashlamp/arclamp pumped solid-state lasers. The ds / dT TL T shows a very intriguing trend as the temperature rises. It presents a minimum of 16 1 107 K1 at 125 K tending to zero as the temperature approaches 225 K, and then inverting its signal and increasing its value up to 300 K, at which ds / dT TL = 1.10 0.08 106 K1. On the other hand, ds / dT OI shows a different tendency, increasing from 6.0 0.3 106 K1 at 50 K to 10.6 0.5 106 K1 at 300 K. In fact, the difference between ds / dT OI and ds / dT TL can be used to calculate additional thermo-optical properties for the sample. These parameters can be related as ds dT ds dT

TL

=
OI

n 1

Then, T T can be calculated. The results are shown in Fig. 6 a open circles . In this calculations we used n = 1.555 and = 0.24.15 The thermal expansion coefcient originates from vibrational anharmonicity in the potential energy and it is usually measured by the Grneisen parameter.11,31 As the temperature decreases, vibrational modes in the higher energy states freeze out and their contribution to the thermal expansion decreases. At high temperatures, there are additional occupants of other vibrational states that contribute to the thermal expansion. The value for the T at 300 K was 11.0 0.8 106 K1, which is in good agreement with the literature value for this glass.15 The results presented above can also be used to determine the temperature dependence of the temperature coef-

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(a)
(10 K )

IV. CONCLUSIONS
25
(10 K )
-6

10 8 6 4 -5 -6 -7 -8

-6

20 15 10

(b)
100 150 200 250 300

Temperature (K)

FIG. 6. Temperature dependence of a the linear thermal expansion coefcient and thermal coefcient of the electronic polarizability and b the temperature coefcient of the refractive index.

In conclusion, this work describes low temperature measurements of the thermal and optical properties of Q-98 phosphate glass. The TL method was used together with the OI and specic heat measurement methods. Our results showed a decrease in the thermal diffusivity with the temperature rise, with a T0.56 dependence between 50 and 130 K and T0.77 between 130 and 300 K. We observed that ds / dT TL T measured via TL technique presented negative values for temperatures below 225 K and positive ones above that. In addition, it is zero at 225 K, temperature in which the glass presents athermal behavior. Finally, the results of this work showed once again that the time resolved TL can be used to determine the thermo-optical properties of glasses at low temperature, providing a differentiation between the changes in the optical path according to the nature of the employed excitation.
ACKNOWLEDGMENTS

cient of the electronic polarizability, T . According to Prodhomme,32 the temperature coefcient of refractive index dn / dT is given by n 1 n +2 dn = dT 6n
2 2

dn/dT (10 K )

-6

-1

-1

-1

8 can be deter-

Substituting dn / dT of Eq. 8 into Eq. 5 , mined as follows: 6n =3 T+ 2 n 1 n2 + 2 ds dT n


OI T

The authors are thankful to the Brazilian Agencies FAPESP, CAPES, CNPq, and Fundao Araucria for the nancial support of this work. The authors would like to thank M. Myers and J. Myers, Kigre Inc., for providing the Q-98 glass sample.
J. H. Campbell and T. I. Suratwala, J. Non-Cryst. Solids 263264, 318 2000 . 2 S. Paoloni, J. Hein, T. Topfer, H. G. Walther, R. Sauerbrey, D. Ehrt, and W. Wintzer, Appl. Phys. B: Lasers Opt. 78, 415 2004 . 3 C. Honninger, F. Morier-Genoud, M. Moser, U. Keller, L. R. Brovelli, and C. Harder, Opt. Lett. 23, 126 1998 . 4 H. Liu, S. Biswal, J. Paye, J. Nees, G. Mourou, C. Honninger, and U. Keller, Opt. Lett. 24, 917 1999 . 5 C. Jacinto, S. L. Oliveira, L. A. O. Nunes, T. Catunda, and M. J. V. Bell, Appl. Phys. Lett. 86, 071911 2005 . 6 D. Jaque, J. C. Lagomacini, C. Jacinto, and T. Catunda, Appl. Phys. Lett. 89, 121101 2006 . 7 N. G. C. Astrath, J. H. Rohling, A. C. Bento, M. L. Baesso, C. Jacinto, S. M. Lima, L. A. O. Nunes, and T. Catunda, J. Phys. IV 125, 185 2005 . 8 A. A. Andrade, T. Catunda, R. Lebullenger, A. C. Hernandes, and M. L. Baesso, J. Non-Cryst. Solids 284, 255 2001 . 9 S. M. Lima, A. A. Andrade, R. Lebullenger, A. C. Hernandes, T. Catunda, and M. L. Baesso, Appl. Phys. Lett. 78, 3220 2001 . 10 C. N. Danson, J. Collier, D. Neely, L. J. Barzanti, A. Damerell, C. B. Edwards, M. H. R. Hutchinson, M. H. Key, P. A. Norreys, D. A. Pepler, I. N. Ross, P. F. Taday, W. T. Toner, M. Trentelman, F. N. Walsh, T. B. Winstone, and R. W. W. Wyatt, J. Mod. Opt. 45, 1653 1998 . 11 N. G. C. Astrath, L. C. Malacarne, P. R. B. Pedreira, A. C. Bento, M. L. Baesso, and J. Shen, Appl. Phys. Lett. 91, 191908 2007 . 12 C. Jacinto, D. N. Messias, A. A. Andrade, S. M. Lima, M. L. Baesso, and T. Catunda, J. Non-Cryst. Solids 352, 3582 2006 . 13 B. D. Sinclair, Opt. Mater. Amsterdam, Neth. 11, 217 1999 . 14 A. J. Kemp, A. J. Maclean, J. E. Hastie, S. A. Smith, J.-M. Hopkins, S. Calvez, G. J. Valentine, M. D. Dawson, and D. Burns, Appl. Phys. B: Lasers Opt. 83, 189 2006 . 15 D. N. Messias, C. Jacinto, M. J. V. Bell, and T. Catunda, IEEE J. Quantum Electron. 43, 0018 2007 . 16 N. G. C. Astrath, J. H. Rohling, A. N. Medina, A. C. Bento, M. L. Baesso, C. Jacinto, T. Catunda, S. M. Lima, F. G. Gandra, M.J. V. Bell, V. Anjos, Phys. Rev. B 71, 214202 2005 . 17 N. G. C. Astrath, A. N. Medina, A. C. Bento, C. Jacinto, T. Catunda, S. M. Lima, L. M. da Silva, F. G. Gandra, and M. L. Baesso, J. Non-Cryst. Solids 354, 574 2008 . 18 M. L. Baesso, J. Shen, and R. D. Snock, J. Appl. Phys. 75, 3732 1994 . 19 S. M. Lima, T. Catunda, R. Lebullenger, A. C. Hernandes, M. L. Baesso, A. C. Bento, and L. C. M. Miranda, Phys. Rev. B 60, 15173 1999 .
1

The results for T Eq. 8 and dn / dT T Eq. 8 are shown in Figs. 6 a and 6 b , respectively. Campbell and Suratwal1 showed that could be considered as an additive contribution from each glass component. Furthermore, Izumitani and Toratoni33 after analyzing several glasses composition observed that is related to the electronic polarizing power of the network forming ions, described by the eld strength Z / a2, with a as the interionic distance in the dipoles and Z its total charge. They observed that a decrease in the eld strength produces an increase in the values, indicating that the elongation of the interionic distance determines . Therefore, because the distance a is expected to increase as the temperature increases, the eld strength decreases. As a consequence, goes to higher values as the temperature increases, similarly to what is observed for T T . Although T increases with the temperature, similarly to T T , they present different temperature dependences. As a result, dn / dT T presents a minimum around the temperature in which ds / dT TL goes to zero, as shown in Fig. 6 b . Finally, the studied glass presents low ds / dT TL value at room temperature, 1 106 K1, and even more interesting, ds / dT TL 0 around 225 K. Low ds / dT value is desired for optical applications. The importance of the athermal characteristics of a material in laser optics depends on how it is excited reinforcing that a complete thermo-optical characterization as the one presented in this work may be useful to understand the physical properties of laser hosts. The athermal behavior for the ds / dT TL is important for laser excited host materials.

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